CN113941320B - Crystalline silicon nanosheet film photoelectrode and preparation method thereof - Google Patents

Crystalline silicon nanosheet film photoelectrode and preparation method thereof Download PDF

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CN113941320B
CN113941320B CN202111210340.3A CN202111210340A CN113941320B CN 113941320 B CN113941320 B CN 113941320B CN 202111210340 A CN202111210340 A CN 202111210340A CN 113941320 B CN113941320 B CN 113941320B
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crystalline silicon
silicon nano
photoelectrode
conductive glass
film
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CN113941320A (en
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吴玉程
蔡蕊
王岩
余翠平
崔接武
张勇
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Hefei University of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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    • B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
    • B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/33—Electric or magnetic properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39—Photocatalytic properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
    • B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
    • B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
    • B01J37/348—Electrochemical processes, e.g. electrochemical deposition or anodisation

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Abstract

The invention discloses a crystalline silicon nano sheet film photoelectrode and a preparation method thereof, which consists of conductive glass and a crystalline silicon nano sheet film deposited on the surface of the conductive glass, wherein the film is prepared by two steps of ultrasonic stripping and electrophoretic deposition by taking crystalline silicon particles as raw materials, ethanol as a solvent and polyvinylpyrrolidone as an additive. The invention has simple operation flow, low cost of raw materials and equipment, and compared with the existing silicon-based photoelectrode, the obtained crystalline silicon nanosheet thin-film photoelectrode has completely different morphological structure characteristics, has better photocurrent response performance under simulated sunlight irradiation, and is a brand-new photoelectrocatalysis material.

Description

Crystalline silicon nanosheet film photoelectrode and preparation method thereof
Technical Field
The invention belongs to the fields of semiconductor technology, micro-nano functional material preparation technology and photoelectrochemical materials, and particularly relates to a thin film photoelectrode consisting of ultrathin crystalline silicon nanosheets and a preparation method thereof.
Background
Realizing the goals of carbon reaching peak and carbon neutralization requires technological innovation in the field of energy of powerful propulsion in China, and developing renewable energy technology. The photoelectrocatalysis of the semiconductor photoelectrode can be used for converting solar energy into clean fuel, so that the storage and conversion of the solar energy are realized, and the method is one of the most valuable renewable energy technologies.
The core of developing the semiconductor photoelectrocatalysis technology is to develop a photoelectrocatalysis material, and the silicon-based film material has excellent light absorption capacity and low material cost, so that the silicon-based film material is one of ideal candidate materials of the photoelectrocatalysis technology. However, the silicon-based thin film materials currently studied are mainly amorphous silicon thin films prepared by vapor deposition methods (such as chinese patent CN201210529409.3, chinese patent CN201410200736.3, etc.). In contrast, a crystalline silicon thin film having a certain crystallinity is advantageous for the transport of photogenerated electrons because of fewer crystal defects, and theoretically has higher solar energy conversion efficiency than an amorphous silicon thin film. However, there are few studies on crystalline silicon films, and the preparation method is mainly based on vapor deposition and amorphous silicon film conversion (such as chinese patent CN200710149348.7, chinese patent CN201310474882.0, chinese patent CN201610232242.2, etc.). The silicon nanocrystals grown by the method have smaller size, uncontrollable morphology, lower crystallization proportion and higher preparation cost.
Compared with amorphous silicon and common polysilicon, the crystalline silicon nano-sheet with the two-dimensional sheet structure has the advantages of adjustable energy band structure, excellent light absorption capacity, high carrier mobility, large specific surface area and the like, and has great application potential in the field of solar photoelectrocatalysis. However, at present, no related research report on photoelectrodes based on crystalline silicon nanoplatelets exists at home and abroad, and the research report mainly has two reasons: firstly, the preparation technology of the silicon nano-sheet is lack, and the batch preparation can be realized; secondly, the product obtained by the existing silicon nano-sheet preparation method is mainly silicon nano-sheet powder, and is used for photoelectrodes, and the product needs to be further prepared into uniform and compact films.
Disclosure of Invention
In order to develop a silicon-based thin film material based on crystalline silicon nano-sheets and expand the application field of the crystalline silicon nano-sheets, the invention aims at the problems, firstly, adopts a liquid phase stripping method with simple process and low cost to prepare the ultrathin crystalline silicon nano-sheets, combines an electrophoretic deposition method on the basis, deposits the ultrathin crystalline silicon nano-sheets obtained by liquid phase stripping on a conductive glass substrate to form uniform and compact crystalline silicon nano-sheet thin films, and prepares the crystalline silicon nano-sheet thin film photoelectrode. Compared with the existing silicon-based photoelectrode, the crystalline silicon nanosheet thin-film photoelectrode has completely different morphological structure characteristics, shows better photocurrent response performance under simulated sunlight irradiation, and is a brand-new photoelectrocatalysis material.
The technical scheme adopted by the invention is as follows:
the invention discloses a crystalline silicon nano sheet film photoelectrode, which is characterized in that: consists of conductive glass and crystalline silicon nano sheet film deposited on the surface of the conductive glass. The crystalline silicon nano sheet film consists of crystalline silicon nano sheets, wherein the transverse dimension of the crystalline silicon nano sheets is 50-3000 nanometers, and the thickness of the crystalline silicon nano sheets is 2-30 nanometers.
The invention also discloses a preparation method of the crystalline silicon nano sheet film photoelectrode, which is prepared by taking crystalline silicon particles as raw materials, ethanol as a solvent and polyvinylpyrrolidone as an additive through two steps of ultrasonic stripping and electrophoretic deposition. The method specifically comprises the following steps:
(1) Adding crystalline silicon particles into an ethanol solvent, carrying out ultrasonic stripping, standing, and taking supernatant to obtain a crystalline silicon nanosheet suspension; then adding polyvinylpyrrolidone into the crystalline silicon nanosheet suspension, and uniformly mixing by ultrasonic to obtain an electrophoresis solution;
(2) And respectively inserting two pieces of conductive glass as an anode and a cathode into the electrophoresis solution in parallel, applying direct-current voltage for deposition, taking out, naturally airing, and annealing to obtain the crystalline silicon nano-sheet film photoelectrode.
Further, the crystalline silicon particles have a size of 50 to 500 μm.
Further, the concentration of the crystalline silicon particles in the ethanol solvent is 5-20 g/l.
Further, the polyvinylpyrrolidone is PVP-K30, and the addition amount is 0.1-0.5wt% of the mass of the crystalline silicon nanosheet suspension;
further, the direct-current voltage is 40-160V, the deposition time is 0.5-3 hours, and the crystalline silicon nano sheet film is deposited on the anode conductive glass.
Further, the annealing is performed under argon or vacuum for 0.5-2 hours at 200-500 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention provides a crystalline silicon nano-sheet film photoelectrode, which is used as a silicon-based film material, and has completely different morphological and structural characteristics compared with the existing amorphous silicon film, silicon nano-film and polysilicon film, wherein the silicon nano-sheet has small thickness, larger transverse dimension and better crystallinity, and in addition, the crystalline silicon nano-sheet photoelectrode also has the unique advantages of a two-dimensional material, such as high carrier mobility, large specific surface area and the like.
2. The invention provides a preparation method of a crystalline silicon nanosheet film photoelectrode, which is prepared by two steps of ultrasonic stripping and electrophoretic deposition, and can be prepared at normal temperature and normal pressure.
3. The silicon nano-sheet reported in the literature is mainly applied to the fields of lithium ion batteries, photoluminescence and photocatalysis hydrogen production. The invention provides the silicon nano-sheet for preparing the silicon-based thin film photoelectrode, expands the application field of the crystalline silicon nano-sheet, and the crystalline silicon nano-sheet thin film photoelectrode shows better photocurrent response performance under the irradiation of simulated sunlight, which indicates that the crystalline silicon nano-sheet is a better photoelectrode material and can be used in the fields of photoelectrocatalysis energy conversion, photoelectric detection and the like.
Drawings
FIG. 1 is a schematic diagram of a process for preparing a crystalline silicon nanosheet thin film photoelectrode according to the present invention.
Fig. 2 is a transmission electron microscope image of the crystalline silicon nanoplatelets prepared by liquid phase exfoliation in example 1.
Fig. 3 is an atomic force microscope image of the crystalline silicon nanoplatelets prepared by liquid phase exfoliation in example 1.
Fig. 4 is a scanning electron microscope image of the crystalline silicon nanoplatelet thin film photoelectrode prepared in example 1 at two magnifications.
Fig. 5 is a scanning electron microscope image of the side of the photoelectrode of the crystalline silicon nanoplatelet film prepared in example 1.
Fig. 6 is a scanning electron microscope image of the crystalline silicon nanoplatelet thin film photoelectrode prepared in example 2 at two magnifications.
FIG. 7 is an X-ray diffraction pattern of the crystalline silicon nanoplatelets thin film photoelectrodes prepared in examples 1-3.
FIG. 8 is a Raman spectrum of the crystalline silicon nanoplatelet thin film photoelectrode prepared in examples 1 to 3.
Fig. 9 is a photocurrent response curve of the crystalline silicon nanoplatelet thin film photoelectrode prepared in example 1 under irradiation of simulated sunlight.
FIG. 10 is a photograph showing the photo of the crystalline silicon nanoplatelets film photoelectrode prepared in examples 1 to 3.
Detailed Description
In order that the above objects, features and advantages of the invention will be readily understood, a more particular description of the invention will be rendered by reference to the appended drawings. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. The invention may be embodied in many other forms than described herein and similarly modified by those skilled in the art without departing from the spirit or scope of the invention, which is therefore not limited to the specific embodiments disclosed below.
The crystalline silicon particles used in the examples below were commercial crystalline silicon particles having a purity of 99.99% and a size of 50 to 500. Mu.m.
Example 1
(1) Adding crystalline silicon particles into 500 ml of ethanol solvent according to the concentration of 5 g/L, carrying out 300W ultrasonic treatment for 12 hours, standing for 12 hours, and taking supernatant to obtain crystalline silicon nanosheet suspension. Fig. 2 is a transmission electron microscope image thereof, from which it can be seen that the product in suspension has an obvious lamellar structure with a lateral dimension of several hundred nanometers, and these lamellar products are silicon nanoplatelets obtained after ultrasonic exfoliation, and fig. 3 is an atomic force microscope image thereof, from which it can be seen that the nanoplatelets have a thickness of 2-3 nanometers, demonstrating that ultra-thin silicon nanoplatelets are obtained by liquid phase exfoliation.
Polyvinylpyrrolidone (PVP-K30) is added into 60 ml of silicon nano-sheet suspension, the addition amount is 0.2% of the mass of the crystalline silicon nano-sheet suspension, and the mixture is subjected to ultrasonic treatment for 1 hour to be uniformly mixed, so that an electrophoresis solution is obtained.
(2) And respectively inserting two pieces of conductive glass with the length of 1cm multiplied by 2cm into an electrophoresis solution in parallel as an anode and a cathode, applying 80V direct current voltage, taking out after 2 hours, naturally airing, and annealing for 2 hours at 300 ℃ under vacuum condition to obtain the crystalline silicon nano sheet film photoelectrode.
FIG. 4 is a scanning electron microscope image of the crystalline silicon nanoplatelet thin film photoelectrode prepared in this example at two magnifications, and it can be seen that a large number of silicon nanoplatelets are uniformly and densely deposited on a conductive glass substrate; fig. 5 is a scanning electron microscope image of the photoelectrode side of the crystalline silicon nanoplatelet film prepared in this example, and it can be seen that the thickness of the film is between 400 and 600 nm. This demonstrates the success of the silicon nanoplatelet films produced by electrophoretic deposition.
Fig. 7 provides an X-ray diffraction pattern of the crystalline silicon nano-sheet film prepared in this example, and it can be seen that there is a distinct diffraction peak at about 28 ° except for the diffraction peak of the FTO conductive glass substrate, which is a diffraction peak corresponding to the (111) crystal plane of crystalline silicon, which indicates that the film has better crystallinity.
FIG. 8 provides a Raman spectrum of the crystalline silicon nanoplatelets film prepared in this example, which can be seen at a wavenumber of 523cm -1 There is a distinct raman peak, which is consistent with the raman characteristic peak of crystalline silicon, further proving that the prepared crystalline silicon nano-sheet film has good crystallinity.
FIG. 9 is a graph showing the response of the photo-electrode of crystalline silicon nanoplatelet film prepared in this example to photocurrent under irradiation of simulated sunlight, which was accomplished in a three-electrode system using an electrochemical workstation, using the photo-electrode of crystalline silicon nanoplatelet film as the working electrode, a platinum sheet as the counter electrode, silver/silver chloride as the reference electrode, 0.5M sodium sulfate as the electrolyte, and 0V vs. RHE as the test voltage, using a xenon lamp light source equipped with a simulated sunlight filter, with an illumination intensity of 100mW/cm 2 . The interval between switching the light source on and off each time for the test was 20 seconds. As can be seen from the figure, under illuminationWhen the current density of the electrode can reach-0.072 mA/cm 2 About, the current density of the electrode is about-0.052 mA/cm when no light is applied 2 About, this indicates that the crystalline silicon nanoplatelet photoelectrode is capable of producing about 0.020mA/cm under the above experimental conditions 2 Shows a good photoelectric response characteristic.
Fig. 10 provides a physical photograph of the crystalline silicon nano-sheet thin film photoelectrode prepared in this example, and it can be seen that a relatively uniform and compact silicon nano-sheet thin film is formed on the surface of the conductive glass through electrophoretic deposition, and the prepared silicon nano-sheet thin film has a gray brown color.
Example 2
(1) Adding crystalline silicon particles into 500 ml of ethanol solvent according to the concentration of 10 g/L, carrying out 350W ultrasonic treatment for 10 hours, standing for 12 hours, and taking supernatant to obtain crystalline silicon nanosheet suspension; polyvinylpyrrolidone (PVP-K30) is added into 60 ml of silicon nano-sheet suspension, the addition amount is 0.1% of the mass of the crystalline silicon nano-sheet suspension, and the mixture is subjected to ultrasonic treatment for 1 hour to be uniformly mixed, so that an electrophoresis solution is obtained.
(2) And respectively inserting two pieces of conductive glass with the length of 1cm multiplied by 2cm into an electrophoresis solution in parallel as an anode and a cathode, applying 40V direct current voltage, taking out after 1.5 hours, naturally airing, and annealing for 1 hour at 400 ℃ under the protection of argon to obtain the crystalline silicon nano sheet film photoelectrode.
Fig. 6 provides scanning electron microscope images of the crystalline silicon nanoplatelet thin film photoelectrode prepared in this example at two magnifications, and it can also be seen that a large number of silicon nanoplatelets are uniformly and densely deposited on a conductive glass substrate. Fig. 7 provides an X-ray diffraction pattern of the crystalline silicon nanoplatelet film prepared in this example. Fig. 8 provides a raman spectrum of the crystalline silicon nanoplatelet film prepared in this example. Fig. 10 provides a physical photograph of the crystalline silicon nanoplatelet thin film photoelectrode prepared in this example.
Example 3
(1) Adding crystalline silicon particles into 1 liter of ethanol solvent according to the concentration of 20 g/liter, carrying out 450W ultrasonic treatment for 6 hours, standing for 24 hours, and taking supernatant to obtain silicon nanosheet suspension; polyvinylpyrrolidone (PVP-K30) is added into 60 ml of silicon nano-sheet suspension, the addition amount is 0.3% of the mass of the crystalline silicon nano-sheet suspension, and the mixture is subjected to ultrasonic treatment for 1 hour to be uniformly mixed, so that an electrophoresis solution is obtained.
(2) And respectively inserting two pieces of conductive glass with the length of 1cm multiplied by 2cm into an electrophoresis solution in parallel as an anode and a cathode, applying 120V direct current voltage, taking out after 1 hour, naturally airing, and annealing for 2 hours at 400 ℃ under a vacuum condition to obtain the crystalline silicon nano sheet film photoelectrode.
Fig. 7 provides an X-ray diffraction pattern of the crystalline silicon nanoplatelet film prepared in this example. Fig. 8 provides a raman spectrum of the crystalline silicon nanoplatelet film prepared in this example. Fig. 10 provides a physical photograph of the crystalline silicon nanoplatelet thin film photoelectrode prepared in this example.
The foregoing is illustrative only and is not intended to limit the present invention, and any modifications, equivalents, improvements and modifications falling within the spirit and principles of the invention are intended to be included within the scope of the present invention.

Claims (6)

1. The preparation method of the crystalline silicon nano sheet film photoelectrode is characterized by comprising the following steps:
(1) Adding crystalline silicon particles into an ethanol solvent, carrying out ultrasonic stripping, standing, and taking supernatant to obtain a crystalline silicon nanosheet suspension; then adding polyvinylpyrrolidone into the crystalline silicon nanosheet suspension, and uniformly mixing by ultrasonic to obtain an electrophoresis solution;
(2) Respectively inserting two pieces of conductive glass as an anode and a cathode in parallel into an electrophoresis solution, applying direct-current voltage for deposition, taking out, naturally airing, and annealing to obtain a crystalline silicon nano-sheet film photoelectrode consisting of the conductive glass and a crystalline silicon nano-sheet film deposited on the surface of the conductive glass; the crystalline silicon nano sheet film consists of crystalline silicon nano sheets, wherein the transverse dimension of the crystalline silicon nano sheets is 50-3000 nanometers, and the thickness of the crystalline silicon nano sheets is 2-30 nanometers.
2. The method of manufacturing according to claim 1, characterized in that: the crystalline silicon particles have a size of 50-500 microns.
3. The method of manufacturing according to claim 1, characterized in that: the concentration of the crystalline silicon particles in the ethanol solvent is 5-20 g/l.
4. The method of manufacturing according to claim 1, characterized in that: the polyvinylpyrrolidone is PVP-K30, and the addition amount is 0.1-0.5wt% of the mass of the crystalline silicon nanosheet suspension.
5. The method of manufacturing according to claim 1, characterized in that: the direct current voltage is 40-160V, the deposition time is 0.5-3 hours, and the crystalline silicon nano sheet film is deposited on the anode conductive glass.
6. The method of manufacturing according to claim 1, characterized in that: the annealing is performed under argon or vacuum for 0.5-2 hours at 200-500 ℃.
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